Five years of scanning electrochemical cell microscopy (SECCM): new insights and innovations

Gaudin, Lachlan F.; Wright, India R.; Harris-Lee, Thom R.; Jayamaha, Gunani; Kang, Minkyung; Bentley, Cameron L.

doi:10.1039/d4nr00859f

Nanoscale

2024

DOI: 10.1039/d4nr00859f

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Five years of scanning electrochemical cell microscopy (SECCM): new insights and innovations

Lachlan F. Gaudin,

India R. Wright,

Thom R. Harris-Lee

et al.

Abstract: Scanning electrochemical cell microscopy (SECCM) is a nanopipette-based technique which enables measurement of localised electrochemistry. SECCM has found use in a wide range of electrochemical applications, and due to the...

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Cited by 4 publications

References 167 publications

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Single‐Entity Electrochemistry of N‐Doped Graphene Oxide Nanostructures for Improved Kinetics of Vanadyl Oxidation

de Oliveira,

Brunet Cabré,

Schröder

et al. 2024

Small

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N‐doped graphene oxides (GO) are nanomaterials of interest as building blocks for 3D electrode architectures for vanadium redox flow battery applications. N‐ and O‐functionalities have been reported to increase charge transfer rates for vanadium redox couples. However, GO synthesis typically yields heterogeneous nanomaterials, making it challenging to understand whether the electrochemical activity of conventional GO electrodes results from a sub‐population of GO entities or sub‐domains. Herein, single‐entity voltammetry studies of vanadyl oxidation at N‐doped GO using scanning electrochemical cell microscopy (SECCM) are reported. The electrochemical response is mapped at sub‐domains within isolated flakes and found to display significant heterogeneity: small active sites are interspersed between relatively large inert sub‐domains. Correlative Raman‐SECCM analysis suggests that defect densities are not useful predictors of activity, while the specific chemical nature of defects might be a more important factor for understanding oxidation rates. Finite element simulations of the electrochemical response suggest that active sub‐domains/sites are smaller than the mean inter‐defect distance estimated from Raman spectra but can display very fast heterogeneous rate constants >1 cm s−1. These results indicate that N‐doped GO electrodes can deliver on intrinsic activity requirements set out for the viable performance of vanadium redox flow battery devices.

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Single‐Entity Electrochemistry of N‐Doped Graphene Oxide Nanostructures for Improved Kinetics of Vanadyl Oxidation

de Oliveira,

Brunet Cabré,

Schröder

et al. 2024

Small

View full text Add to dashboard Cite

show abstract

Elucidating the structure–activity relationship on single entities by scanning electrochemical cell microscopy

Zou,

Chen

2024

Current Opinion in Electrochemistry

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In Situ Quantification of a Wetted Surface Area during Scanning Electrochemical Cell Microscopy Using Retraction Curves

Saxena,

Mena-Morcillo,

Tripp

et al. 2024

ACS Meas. Sci. Au

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This work presents a new methodology to estimate the surface area of the working electrode during scanning electrochemical cell microscopy (SECCM) in situ by utilizing retraction curves. In this approach, the current is measured as a function of pipet displacement in the z-direction. When the current drops to zero, it is indicative of droplet detachment from the surface, allowing for the estimation of the droplet contact diameter based on the pipet displacement. This enables real-time estimations of surface areas of the wetted electrode at each point of measurement, rather than performing time-consuming measurements using ex situ correlative image analysis or estimating an average working electrode size from the pipet aperture. Notably, during SECCM measurements on copper in nitric acid, the working electrode diameter estimated using retraction curves was significantly smaller than the droplet footprint diameter observed post experiment using ex situ correlative image analysis. This discrepancy is attributed to droplet spreading after pipet retraction, as confirmed by goniometer and silanized pipet measurements. Upon cleaning the surface, the true wetted surface areas during SECCM measurements were found to be in good agreement with values estimated using retraction curves yet were larger than the pipet aperture. Additionally, the effects of approach separation, retraction rates, and probe diameter on the droplet contact size were analyzed using retraction curves. These findings were compared to ex situ methods to assess the reliability of the retraction curves for determining the working electrode surface area. This study demonstrates the potential of retraction curves to provide a higher accuracy in the quantitative analysis of local current density values extracted using SECCM.

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Five years of scanning electrochemical cell microscopy (SECCM): new insights and innovations

Abstract: Scanning electrochemical cell microscopy (SECCM) is a nanopipette-based technique which enables measurement of localised electrochemistry. SECCM has found use in a wide range of electrochemical applications, and due to the...

Cited by 4 publications

References 167 publications

Single‐Entity Electrochemistry of N‐Doped Graphene Oxide Nanostructures for Improved Kinetics of Vanadyl Oxidation

Single‐Entity Electrochemistry of N‐Doped Graphene Oxide Nanostructures for Improved Kinetics of Vanadyl Oxidation

Elucidating the structure–activity relationship on single entities by scanning electrochemical cell microscopy

In Situ Quantification of a Wetted Surface Area during Scanning Electrochemical Cell Microscopy Using Retraction Curves

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